.beta.-D-Ribofuranoside, methyl 2,3-O-(1-methylethylidene)-, 5-(4-methylbenzenesulfonate)

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

February 22, 2005 to June16, 2005

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: see 'Remark'

Remarks:

EEC Directive 92/69, Part A, Methods for the determination of physico-chemical properties, A.1 “Melting/Freezing temperature”, EEC Publication No. L383, December 1992. OECD Guideline for Testing of Chemicals No. 102, “Melting Point / Melting Range”, adopted July 27, 1995.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2005

Report date:

2005

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Test material

Test material information

Constituent 1

Reference substance name:

[(3aS,4S,6S)-6-methoxy-2,2-dimethyl-tetrahydro-2H-furo[3,4-d][1,3]dioxol-4-yl]methyl 4-methylbenzene-1-sulfonate

EC Number:

609-920-2

Cas Number:

4137-56-8

Molecular formula:

C16H22O7S

IUPAC Name:

[(3aS,4S,6S)-6-methoxy-2,2-dimethyl-tetrahydro-2H-furo[3,4-d][1,3]dioxol-4-yl]methyl 4-methylbenzene-1-sulfonate

Details on test material:

Identity: Tosylfuranosid
Appearance: Solid / white
Storage: At room temperature at about 20°C
Expiration Date: July 31, 2005

Results and discussion

Melting / freezing point

Melting / freezing pt.:

>= 63.2 - <= 336.4 °C

Any other information on results incl. tables

Thermal Analysis

Test System

Instrument: Differential Scanning Calorimeter

DSC 821, Fa. Mettler Toledo

Sample cups: Aluminium cups.

Test conditions: The test was performed in an air atmosphere.

Reference cup: Empty aluminium cup.

Preliminary Test

A test item amount of 4.54 mg was heated up from 25°C to 400°C at a rate of 20 K/min. The quantities of heat absorbed or released were measured and recorded. Before and after the test, the weight and the appearance of the sample were determined.

Main Tests

Melting Point

As in the temperature range investigated a peak was observed from which melting of the sample could be deduced, the thermal analysis was repeated in the immediate vicinity of the peak temperature with the temperature rise adjusted to 10 K/min. For the actual determination of the melting point, 6.17 mg and 6.16 mg of test item were heated up. Before and after the test, the weight and the appearance of the samples were determined.

Applicant's summary and conclusion

Conclusions:

During this study the melting point of Tosylfuranosid was determined.
The mean melting range / point of Tosylfuranosid was determined to be
63.2°C ± 0.5°C which is equal to 336.4 K ± 0.5 K.

Executive summary:

The purpose of the study was to evaluate the melting point / melting range of Tosylfuranosid.

The DSC-curve of the preliminary test (heating rate of 20 K/min from 25°C to 400°C) shoved that the first endothermic heat effect, the melting, was observed at 67.5°C.

Melting Point

In order to determine the melting more precisely, further DSC-runs were recorded between 25°C and 90°C with a heating rate of 10 K/min. In the first main test run, the melting of Tosylfuranosid was determined at 62.9°C. The melting of the test item during the second main test run was determined to be at 63.6°C. During these runs, the samples lost 4.5 % and 4.1 % of their mass, respectively. After the measurement, the residues of both molded samples were clear with a red sheen.

In conclusion, the melting point of Tosylfuranosid was determined to be 63.2°C ± 0.5°C which is equal to 336.4 K ± 0.5 K.